반응 #168799

반응 방정식

sodium hydride

MeOH

3-amino-5-chloro-pyrazine-2-carboxylic acid methyl ester

NH4Cl

→

title compound

3-Amino-1-methoxy-pyrazine-2-carboxylic acid methyl ester

반응 조건

후처리

1. 1
   기타At 0° C
2. 2
   온도After re-cooling to 0° C
3. 3
   온도to warm to room temperature
4. 4
   workup.STIRRINGstirred over night
5. 5
   추출the mixture was extracted with DCM and EtOAc
6. 6
   세척the combined organic layers were washed with saturated aqueous sodium chloride
7. 7
   건조dried with Na2SO4
8. 8
   기타evaporated
9. 9
   기타The residue was purified by chromatography on silica gel (cyclohexane to EtOAc)

실험 절차

At 0° C. 75 mg (1.866 mmol) 60% sodium hydride in oil was added in portions to 5 ml MeOH and the mixture was stirred at room temperature for 30 min. After re-cooling to 0° C. 350 mg (1.866 mmol) 3-amino-5-chloro-pyrazine-2-carboxylic acid methyl ester (GB 1248146) was added and the mixture was allowed to warm to room temperature and stirred over night. Saturated aqueous NH4Cl was added and the mixture was extracted with DCM and EtOAc, the combined organic layers were washed with saturated aqueous sodium chloride, dried with Na2SO4 and evaporated. The residue was purified by chromatography on silica gel (cyclohexane to EtOAc) to provide the title compound as colorless solid.

출처